フェノール溶解法による高純度金属マグネシウム中の酸化マグネシウムの定量

フォーマット:

論文

責任表示:

松本, 健 ; 小泉, 貞之 ; 木羽, 敏泰

言語:

日本語

出版情報:

The Japan Society for Analytical Chemistry = 日本分析化学会, 1979-01-05

著者名:

• 松本, 健
• 小泉, 貞之
• 木羽, 敏泰

掲載情報:

分析化学 = Japan analyst

ISSN:

0525-1931      

巻:

28

通号:

1

開始ページ:

20

終了ページ:

25

バージョン:

publisher

概要:

金沢大学イノベーション創成センター<br />100m1二ロフラスコにフェノール40mlを入れ,予備加熱して脱水してからフラスコ内を窒素ふんい気とした後,試料の高純度マグネシウム片を加え,加熱還流すると,金属はマグネシウムフェノオキシドとなって溶解し,酸化物は溶けないで残さとなる.無水メタノールを加えて希釈後,酸化物残さを濾別し希塩酸で溶解した水溶液について,マグネシウムの量を原子吸光法で定量し酸化物量を求める.本法の精度は高く,金属表面及び内部の酸化物の総量を簡 … 単迅速に定量できる. A 40 ml of phenol was put in 100 ml two neck round-bottom flask equipped with a conventional distillation device and a ground glass stopper, and heated to the boiling point of phenol, 180℃. During this treatment, a slight amount of water contained in phenol was eliminated from phenol as the azeotropic vapor mixture of phenol and water at 99.5℃, and phenol was thoroughly dehydrated. After the distillation device was replaced by a reflux condenser, a piece of magnesium metal sample was put quickly into the flask through the side neck. Then the content was heated under stirring at 180℃, until magnesium metal diminished completely in phenol, forming magnesium phenoxide, while magnesium oxide remained as residue. The reaction mixture was cooled to (50〜60) ℃, and anhydrous methanol was added to keep phenol and magnesium phenoxide in dissolving form. The residual magnesium oxide was caught on a sintered glass filter (1G5) and dissolved in 50 ml of 2 M hydrochloric acid. The solution was diluted to a definite volume and magnesium in the solution was determined by the atomic absorption spectrometry. All the experiments were carried out in a glove box in dry nitrogen atmosphere to avoid the influence of oxygen and water from air. By the above procedure a minute amount of magnesium oxide could be determined precisely with high reproducibility. To clarify the behaviors of magnesium metal and magnesium oxide in this separation process additional experiments were also done. 続きを見る

URL:

http://hdl.handle.net/2297/24892